関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Ethylpyrazolo[1,5-a]pyridine-3-carboxylic acid | HCID 58379320 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Ethylpyrazolo[1,5-a]pyridine | HCID 16116261 | 82% |
反応手順
2-Ethylpyrazolo[1,5-a]pyridine-3-carboxylic acid (4.1 g, 22 mmol) was stirred in water (100 mL) and sulfuric acid (2.5 mL) was added. The mixture was heated at 70° C. for 2 h and cooled to 20° C. The mixture was poured into ethyl acetate and neutralized with saturated sodium bicarbonate. The extracts were separated and the aqueous layer was extracted with ethyl acetate. The combined extracts were dried (sodium sulfate) and evaporated to give the desired compound (2.6 g, 82%). LCMS for C9H11N2 (M+H)+: m/z=147.1. 1H NMR (300 MHz, DMSO-d6): δ 8.52 (m, 1H), 7.57 (m, 1H), 7.11 (m, 1H), 6.75 (m, 1H), 6.38 (s, 1H), 2.73 (m, 2H), 1.22 (m, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08759359B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-dff0416bf98646839691f01d002b0f15 |
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| 出典メモ | uspto-grants-2014_06 |
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